Microemulsions for high viscosity amino silicone fluids and gums and their preparation

ABSTRACT

Microemulsion compositions comprising microemulsifiable high viscosity amino silicone fluids or gums and a surfactant having a high phase inversion temperature, the microemulsions formed therewith, a means for preparing said microemulsions, and personal care products comprising said microemulsions.

CROSS-REFERENCE TO RELATED APPLICATIONS

This is a continuation-in-part of copending application Ser. No. 08/250filed on May 27, 1994.

FIELD OF THE INVENTION

The instant invention comprises a method for preparing microemulsions.The process of the invention comprises blending a high viscosity aminosilicone fluid or gum with a surfactant having a high phase inversiontemperature adding an approximately equal amount of water at atemperature approximately equal to the phase inversion temperature ofthe surfactant, acidifying, followed by rapidly adding water. Theinstant invention further comprises personal care products comprisingthe microemulsion prepared by the process of the invention.

BACKGROUND OF THE INVENTION

The instant invention is related to a method of making microemulsionblends having an average particle size of from about 0.001 microns toabout 0.05 microns whereby the blend comprises at least one low aminocontent silicone and a surfactant having a high phase inversiontemperature. The instant invention is further related to personal careproducts comprising said microemulsion.

Microemulsions containing silicone fluids have been found to be usefulin a variety, of personal care products. As defined herein, the term"microemulsions" refers to transparent mechanically and thermally stablesystems comprising small droplets having a mean or average particlediameter usually not more than 0.05 microns in diameter, preferably notmore than 0.040 microns in diameter and most preferably not more than0.025 microns in diameter. The small size of the droplets imparts a highdegree of transparency to the emulsion.

The use of microemulsions is known in the art, see for example U.S. Pat.No. 4,797,272 (Linnet al.) and U.S. Pat. No. 4,620,878 (Gee). U.S. Pat.No. 4,797,272 to Linnet al. discloses water-in-oil microemulsioncompositions having a mean droplet size ranging from about 0.001 micronsto about 0.200 microns. U.S. Pat. No. 4,620,878 to Gee discloses apolyorganosiloxane emulsion that contains a polyorganosiloxanecontaining at least one polar radical such as an amino or ammoniumradical attached to the silicon of the siloxane by Si--C or Si--O--Cbonds or at least one silanol radical and at least one surfactant thatis insoluble in the polyorganosiloxane. Water is added forming atranslucent oil concentrate. The translucent oil concentrate is thenrapidly dispersed in water to prepare emulsions with fairly low particlesizes. A drawback of Gee's teachings is that the oil concentrate must bediluted with very large quantities of water such that the final emulsionrarely contains more than about 5 wt. % silicone solids. The emulsionsprepared by Gee typically have an average particle size of less than0.14 microns.

Microemulsions of volatile silicones are taught in the art, for exampleU.S. Pat. No. 4,782,095 and U.S. Pat. No. 4,801,447, however thesemicroemulsions have required large amounts of surfactants. The highlevels of surfactants required in the prior art applications aredetrimental in many applications.

Chrobaczek and Tschida in U.S. Pat. 5,057,572 teach the preparation ofan aminoalkyl substituted polysiloxane where the silicone fluid, awater-soluble emulsifier, in contrast to Gee, water and an acid arecombined and heated to 50° C. The necessity, for a specific sequence ofprocess steps, such as order of addition, is not taught by Chrobaczek.While Chrobaczek teaches this procedure is applicable to silicone fluidswith an amino content of 0.1 meq./gr., in practice microemulsions resultonly when the amino content is above a threshold of about 0.12 to 0.14meq./gr. Below this threshold level the particle size of the emulsion issuch that the emulsion is hazy, and therefore not a true microemulsion,true microemulsions possess optical transparency to a greater or lesserdegree, as measured by an ASTM haze number of less than about 150.

Breneman et al. in U.S. Pat. No. 5,234,495 teach the preparation ofmicroemulsions through a process utilizing the blending of an organomodified polysiloxane, e.g. an aminofunctional polysiloxane, an organomodified polysiloxane emulsifier, water, and an alkaline metal salt.Heating such a blend above the cloud point of the mixture andsimultaneously subjecting the mixture to high shear mixing produces aliquid phase that can be cooled to form a microemulsion.

Microemulsions of aminofunctional silicones, particularly high viscosityaminofunctional silicone fluids or gums, provide beneficial results whenused in personal care product formulations. It continues to be desirableto provide alternative or improved methods for preparing microemulsionsof small average particle size.

SUMMARY OF THE INVENTION

In one embodiment, the instant invention comprises a transparentoil-in-water microemulsion comprising: (a) a microemulsifiable highviscosity amino silicone fluid or gum, (b) a surfactant having a highphase inversion temperature, and (c) water.

In another aspect, the instant invention provides a method of ispreparing a transparent polyorganosiloxane microemulsion having a meanparticle size of from about 0.001 to about 0.050 microns, preferablyfrom about 0.010 to about 0.030 microns, and most preferably from about0.010 to about 0.025 microns, comprising a microemulsifiable highviscosity amino silicone fluid or gum and at least one surfactant havinga high phase inversion temperature.

Other aspects of the invention are microemulsions ofpolydimethylsiloxane and personal care products comprising themicroemulsions of the present invention.

DETAILED DESCRIPTION OF THE INVENTION

The instant invention is based upon the discovery that functionalizedsilicones such as high viscosity amino functional silicone fluids orgums are capable of forming microemulsions and may be blended withsurfactants having a high phase inversion temperature and the blendprocessed such that the mixture forms a microemulsion. Suchmicroemulsions are generally transparent. By transparent applicants meanthe absence of turbidity or haze wherein haze is defined by an ASTMtest, specifically ASTM test number D871 using turbidity suspensionstandards and wherein said haze or turbidity is below an upper limit ofabout 150. At levels of the haze number above about 50 themicroemulsions of the present invention begin to gradually change fromtransparent to translucent. The haze numbers of the microemulsions ofthe present invention range from 0 to about 150, more preferably fromabout 0 to about 80 and most preferably from 0 to about 50. Theturbidity suspension standards used in the ASTM test D871 are availablefrom Hellige Incorporated of Garden City, N.Y. Applicants note that puredistilled water is 0 on the haze scale.

Polyorganosiloxane microemulsions prepared by the method of the instantinvention have a mean particle size of from about 0.0005 to about 0.050microns, preferably from about 0.010 to about 0.030 microns, and mostpreferably from about 0.010 to about 0.025 microns. Generally haze andaverage particle size correlate with one another but they are alsoaffected by the relative amounts of the two major components of theemulsion, the silicone oil and the water. Thus while at a constant oilto water ratio the haze and average particle size might correlate, hazeby itself is not both a necessary and sufficient criterion to be anindicator of average particle size in a microemulsion unless otherconstraints are specified.

By microemulsifiable applicants define the term to mean capable offorming a microemulsion wherein the mean particle size of the emulsionranges from 0.0001 microns to about 0.050 microns. By microemulsifiablesilicone applicants define a silicone or a mixture of silicones that canform a microemulsion as defined by applicants herein before.

The phase inversion temperature is that temperature at which a givensurfactant is equally soluble in a lipophilic and a hydrophilic phasethat are co-extensive. Generally the hydrophilic phase of interest oruse is water. At the phase inversion temperature, the surfactant,hydrophilic phase and lipophilic phase are in a thermodynamic state ofminimum free energy. This thermodynamic state is characterized by aminimum in particle size of the emulsion formed therewith when themixture is emulsified. Thus the phase inversion temperature has atendency to be specific for a given composition of components. While thephase inversion temperature varies as a function of composition, whenone of the two liquid phases is held constant e.g. water, the phaseinversion temperature of a series of mixtures utilizing a givensurfactant, water, and a variety of lipophilic phases that areimmiscible with the water, the phase inversion temperature will tend tovary over a much narrower range of temperatures.

In one embodiment of the instant invention an oil surfactant mixture isprepared by blending:

(1) an amount ranging from 10 to 30 parts per hundred of the finalcomposition of the microemulsion of a polyorganosiloxane that can bemicroemulsified, A(1), optionally having an amino content of from about0.10 to about 3.0 milliequivalents per gram and comprising a silicone ofthe formula:

    M(R.sub.a Q.sub.b SiO.sub.(4-a-b) /2).sub.x (R.sub.c SiO.sub.(4-c) /2).sub.y M

whereby in the formulas above R is a hydrocarbon or hydrocarbon radicalhaving from 1 to about 6 carbon atoms, Q is a polar radical having thegeneral formula--R¹ HZ, wherein R¹ is a divalent linking group bound tohydrogen and the radical Z, comprised of carbon and hydrogen atoms;carbon, hydrogen and oxygen atoms, or carbon, hydrogen and nitrogenatoms; and Z is an organic amino functional radical containing at leastone amino functionality; "a" assumes values ranging from about 0 toabout 2, "b" assumes values ranging from about 1 to about 3, "a"+"b" isless than or equal to 3, and "c" is a number in the range of from about1 to about 3; and x is a number in the range of from 5 to about 2,000preferably from about 9 to about 500 and most preferably from about 13to about 185, and y is a number in the range of from about 800 to about10,000, preferably from about 1,250 to about 5,000, and most preferablyfrom about 1,500 to about 5,000, and M is any suitable siliconeendstopping group known in the art. Non-limiting examples of radicalsrepresented by R include alkyl radicals such as methyl, ethyl, propyl,isopropyl, butyl, isobutyl, amyl, isoamyl, hexyl, isohexyl, and thelike; alkenyl radicals such as vinyl, halo vinyl, alkyl vinyl, allyl,haloallyl, alkylallyl, cycloalkyl radicals such as cyclobutyl,cyclopentyl, cyclohexyl and the like, phenyl radicals, benzyl radicals,halohydrocarbon radicals such as 3-chloropropyl, 4-bromobutyl,3,3,3-trifluoropropyl, chlorocyclohexyl, bromophenyl, chlorophenyl andthe like, and sulfur containing radicals such as mercaptoethyl,mercaptopropyl, mercaptohexyl, mercaptophenyl and the like; preferably Ris an alkyl radical containing from 1 to about 6 carbon atoms; and mostpreferably R is methyl. Examples of R¹ include methylene, ethylene,propylene, hexamethylene, decamethylene, --CH₂ CH(CH₃)CH₂ --, phenylene,naphthylene, --CH₂ CH₂ SCH₂ CH₂ --, --CH₂ CH₂ OCH₂ --, --OCH₂ CH₂ --,--OCH₂ CH₂ CH₂ --, --CH₂ CH(CH₃)C(O)OCH₂, --(CH₂)₃ CC(O)OCH₂ CH₂ --,--C₆ H₄ C₆ H₄ --, --C₆ H₄ CH₂ C₆ H₄ --, and --(CH₂)₃ C(O)SCH₂ CH₂ --.

Z is an organic am/no functional radical containing at least one aminofunctionality. One possible formula for Z is --NH(CH₂)_(z) NH₂ where zis one or greater. Another possible formula for Z is --N(CH₂)_(z)(CH₂)_(zz) NH where both z and zz are independently one or greater, thisstructure encompasses diamino ring structures such as piperazinyl. Z ismost preferably a --NHCH₂ CH₂ NH₂ radical.

Q is most preferably an amine functional polar radical having theformula --CH₂ CH₂ CH₂ NHCH₂ CH₂ NH₂.

In the formulas, "a" assumes values ranging from about 0 to about 2, "b"assumes values ranging from about 1 to about 3, "a"+"b" is less than orequal to 3, and "c" is a number in the range of from about 1 to about 3.The molar ratio of R_(a) Q_(b) SiO.sub.(4-a-b) /2 units to R_(c)SiO.sub.(4-c) /2 units ranges from about 1:2 to about 1:65, preferablyfrom about 1:5 to about 1:65, and most preferably from about 1:15 toabout 1:20.

It is preferred to use amino functional silicone gums or fluids A(1) inthe instant invention having the formula:

    (CH.sub.3).sub.3 SiO[(CH.sub.3)(C.sub.3 H.sub.6 NH.sub.2 C.sub.2 H.sub.4 NH.sub.2)SiO].sub.x [(CH.sub.3).sub.2 SiO].sub.y Si(CH.sub.3).sub.3

wherein x is a number in the range of from 5 to about 2,000 preferablyfrom about 9 to about 500 and most preferably from about 13 to about185, and y is a number in the range of from about 800 to about 10,000,preferably from about 1,250 to about 5,000, and most preferably fromabout 1,500 to about 5,000, wherein said amino functional silicone fluidor gum has a viscosity ranging from 10,000 to 10,000,000 centistokes at25° C., preferably the viscosity ranges from 10,000 to 2,000,000centistokes, and most preferably the viscosity ranges from 100,000 to2,000,000 centistokes.

(2) adding to the silicone blend from step (1), of from about 1 to 30parts per hundred of the final composition of the microemulsion of atleast one surfactant, A(3), wherein at least one of the surfactants hasa high phase inversion temperature, said phase inversion temperaturegenerally ranging from about 45° to about 95° C.;

(3) heating the blend of silicone(s) and surfactant(s) to a temperatureranging from about 45° C. to about 95°C., which is a temperature belowthe phase inversion temperature of the surfactant(s), while stirring;

(4) water, Part I water in the examples, in an amount equal in weight tothe weight of the silicone(s) used in Part I added slowly;

(5) adding an amount of an acid such that the final pH of themicroemulsion is between about 4 and 7; preferably steps (4) and (5) areaccomplished simultaneously either by the separate addition of water anda suitable acid or by the addition of an aqueous solution of a suitableacid. A preferred acid is acetic acid, however other acids may also beused such as HCl hypophosphorous, lactic, propionic, glycolic, formic,and nitric.

(6) water, Part II water in the examples, in an amount ranging from 40to about 90 parts, said part II water having a temperature ranging from0° C. to about 95° C. below the temperature of acidified emulsion suchthat by the addition of said cold water the temperature of saidmicroemulsion is cooled rapidly. Additionally, Part II water may containa high molecular weight polymer such as polyvinyl alcohol, hydroxymethylcellulose or the like, to improve the stability of the finalemulsion.

A(3) contains at least one surfactant, wherein at least one of thesurfactants has a phase inversion temperature ranging from 50° C. toabout 95° C., said surfactant hereinafter referred to as the primarysurfactant. Other optional surfactants are referred to as secondarysurfactants.

The surfactant or blend of surfactants has a hydrophilic-lipophilicbalance value of from about 10 to about 16, preferably from about 11 toabout 16, and most preferably from about 12 to about 13. The preferredhydrophilic-lipophilic balance value may vary as a consequence ofincreasing the level of volatile silicone in the microemulsifiablesilicone.

The primary surfactant may be cationic, anionic, nonionic or amphotericin nature. Examples of such surfactants are disclosed in U.S. Pat. No.4,620,878 to Gee which is hereby incorporated by reference. Generally,nonionic surfactants are preferred for use in the instant invention.

Surfactants useful as the primary surfactant in the instant inventioninclude the polyoxyethylene sorbitan esters of C₁₀ to C₂₂ fatty acidshaving up to 95% ethylene oxide; polyoxyethylene sorbitol esters of C₁₀to C₂₂ fatty acids, polyoxyethylene derivatives of fatty phenols having6 to 20 carbon atoms up to 95% ethylene oxide; fatty amino and amidobetaines having 10 to 22 carbon atoms, and polyethylene condensates ofC₁₀ to C₂₂ fatty acids or fatty alcohols having up to 95% ethyleneoxide.

Preferred primary surfactants for the practice of the instant inventioninclude, but are not limited to, the alkylphenoxy polyethoxy ethanols,which are nonionic surfactants possessing varying amounts of ethyleneoxide units and are available from Union Carbide Corporation under thegeneral TRITON® trade name; trimethylnonyl polyethylene glycol ethersand polyethylene glycol ethers of 11-15 carbon atom containing alcohols,which may be linear or branched, preferably branched, available fromUnion Carbide Corporation under the general trade name TERGITOL®; thenonionic ethoxylated tridecyl ethers, available from Emery Industriesunder the trade name TRYCOL®.

The preferred surfactants for use as the primary surfactant of theinstant invention are the trimethylnonyl polyethylene glycol ethers andpolyethylene glycol ethers of 11-15 carbon atom containing alcohols,which may be linear or branched, preferably branched, available fromUnion Carbide Corporation under the trade name TERGITOL®. A preferredsurfactant for use as the primary surfactant of the instant invention isa trimethylnonyl polyethylene glycol ether. The most preferred primarysurfactant is 2,6,8-trimethyl-4-nonyloxypolyethylene oxide (TERGITOL®TMN-6)

The optional secondary surfactants may be anionic, cationic, nonionic,or amphoteric and may either be soluble or insoluble in the preferredamino functional silicone of A(1). Nonionic surfactants are preferred.Non-limiting examples of surfactants that are soluble in the aminofunctional silicone include the alkyl phenol ethoxylates. A particularlypreferred optional secondary surfactant is TRITON X-405®.

Preferably, the optional secondary surfactant used in this invention isalso insoluble in the silicone of A(1). The preferred surfactants foruse as the secondary surfactants in the instant invention are the alkylphenoxy polyethoxy ethanols.

The amount of A(3) is in the range of from about 1 to about 30,preferably from about 1 to about 20, and most preferably from about 5 toabout 15, parts by weight per 100 parts by weight of the finalmicroemulsion composition.

The blend of silicones, surfactants and water is homogenized in ahomogenizer or other suitable mixing equipment. The length of timenecessary to form a homogeneous mixture or emulsion in this step willdepend on mixing equipment parameters and can be determined by thoseskilled in the art without undue experimentation. High shear mixing,either at ambient pressure or under conditions where the reaction mediumis pressurized are generally unnecessary in order to form themicroemulsions of the instant invention. Because the blend contains asurfactant having a high phase inversion temperature, the temperature atwhich the microemulsion is formed must be carefully controlled. Thus thestep of adding part I water is performed in a temperature range varyingbetween 45° C. and 95° C., more preferably varying between 55° C. and90° C., and most preferably varying between 65° C. and 85° C.

In step (5) the microemulsion is acidified to bring the pH of theemulsion into a range varying between 4 and 7, more preferably between 5and 6.5, and most preferably between 5.5 and 6.5. This step isparticularly effective when combined with step (4)

In order to change the pH of the reaction medium, it is necessary toconsider the quantity of amino functional silicone or silicone presentin the reaction mixture. The amount of acid needed to provide such pHvalues will depend on the amount of the amino functional silicone orsilicone fluid (A)(1) and the amino content of the amino functionalsilicone fluid. For example, with the amino functional silicone fluidhaving an amino content of 0.6 milliequivalents per gram, the amount ofacid sufficient to provide a pH within the desired range will beapproximately 2.5 parts per weight per 100 parts per weight of the aminofunctional silicone fluid. With an amino functional silicone fluidhaving an amino content of 3.0 milliequivalents per gram, the weight ofacid will be about 1.25 parts per weight per 100 parts per weight of thefluid. While the weights of acid necessary to achieve a given pH mayvary depending on the molecular and equivalent weights of the acidchosen to control the pH, control of pH to the desired value is theprimary purpose of the acid addition. Further, it has been found thatthe addition of acid must be s simultaneous with the addition of thepart I water.

Additionally, silicone fluids, particularly amino or ammonium functionalsilicone fluids, having a viscosity ranging from 10,000 to 10,000,000centistokes at 25° C. are preferred for use with the process of theinstant invention. Thus amino functional silicone fluids having an aminocontent ranging from about 0.10 meq./gr. to about 10.0 meq./gr. andviscosity, ranging from about 10,000 to about 10,000,000 centistokes at25° C. are preferred for use with the process of the instant invention.

The amino functional silicone microemulsions of the present inventionare useful in a variety of personal care product applications is such ashair conditioners, the so-called 2 in 1 shampoos, and hair fixativepreparations such as styling gels mousses and the like. For purposes ofpersonal care applications the conditioner formulations generallycomprise an amino functional silicone microemulsion content ranging fromabout 5 weight percent to about 15 weight percent, more preferably fromabout 5 weight percent to about 10 weight percent, and most preferablyfrom about 6 weight percent to about 7 weight percent. For purposes ofpersonal care applications the 2 in 1 shampoo formulations generallycomprise an amino functional silicone microemulsion content ranging fromabout 2 weight percent to about 7 weight percent, more 25 preferablyfrom about 2 weight percent to about 5 weight percent, and mostpreferably from about 3 weight percent to about 4 weight percent. Forpurposes of personal care applications the fixative formulationsgenerally comprise an amino functional silicone microemulsion contentranging from about 2 weight percent to about 10 weight percent, morepreferably from about 2 weight percent to about 6 weight percent, andmost preferably from about 3 weight percent to about 5 weight percent.The personal care products utilizing microemulsions prepared by theprocess of the instant invention will typically exhibit haze numbersbelow about 100. Applicants note that the weight percent ranges hereinbefore described constitute weight percent ranges for the finishedmicroemulsions as a component of the personal care product. Thus amicroemulsion prepared by the process of the present invention will havea silicone content varying from about 5 weight percent to about 25weight percent, which will vary from about 0.1 weight percent to about 7weight percent as a percentage of the final composition of the personalcare product when the microemulsion is incorporated into the personalcare product. Additionally, the microemulsions of the present inventionmay be formulated into textile heating products or skin careformulations including color cosmetics.

EXPERIMENTAL

The procedure outlined in the detailed description of the invention wasutilized to prepare the following non-limiting examples, examples 1through 24, which are illustrative of the microemulsions of the instantinvention. Uses of these microemulsions in personal care products arealso demonstrated. Examples 39 through 43 are illustrative of personalcare formulations.

EXAMPLE 1

While warming to 70° C., 16 parts of an aminofunctional silicone(linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂,viscosity of 150 to 400 centistokes, amine content of 0.12 meq/gr.) wasmixed with 8 parts TERGITOL TMN-6. Part I water (16 parts) was thenadded dropwise at 70° C. After water addition was complete, 1 part ofacetic acid was added. The mixture thickened and became translucent.Part II water (58 parts) was then added rapidly with good agitation.Upon cooling, a microemulsion having an ATM haze number of about 40 wasobtained.

COMPARATIVE EXAMPLE 1

This example was prepared in the same fashion as Example 6 in U.S. Pat.No. 5,057,572. While warming to 70° C., 16 parts of an aminofunctionalsilicone (linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂--NH₂, viscosity of 150 to 400 centistokes, amine content of 0.12meq/gr.) was mixed with 8 parts TERGITOL TMN-6 and 74 parts water toform a homogeneous mixture. Lactic acid (1 part) was then added at 70°C. After cooling a milky emulsion was obtained. The haze number of thispreparation was greater than 200.

EXAMPLE 2

This example shows the effect of adding part II water slowly. Whilewarming at 70° C., 20 parts of an aminofunctional silicone (linear,trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂, viscosity of150 to 400 centistokes, amine content of 0.12 meq/gr.) was mixed with12.5 parts TERGITOL TMN-6. Part I water was then added dropwise at 70°C. After water addition was complete, 0.5 parts of acetic acid wasadded. The mixture thickened and became translucent. Part II water (53parts) was then added dropwise with good agitation. The mixture slowlybecame thicker and then eventually thinned out towards the end of thewater addition. Upon cooling, a microemulsion with a haze of about 200was obtained.

EXAMPLES 3-7

These examples show the effect of different amounts of part I water (theamounts specified are in grams):

    ______________________________________                                                 Ex.      Ex.    Ex.     Ex.    Ex.                                   Component                                                                              3        4      5       6      7                                     ______________________________________                                        Amino fluid                                                                            65       65      65      65    65                                    A1                                                                            TERGITOL 40       40     40       40     40                                   TMN-6                                                                         Part I Water                                                                           40       65     90      120    220                                   Acetic Acid                                                                            1        1      1        1      1                                    Part II Water                                                                          180      155    1130    100     0                                    Haze     150      30     90      200+   200+                                  pH       5.5      5.5    5.5      5.5   nm                                    ______________________________________                                    

EXAMPLES 8-12

These examples show the effect of different amounts of surfactant (theamounts specified are in grams):

    ______________________________________                                                   Ex.      Ex.    Ex.    Ex.  Ex.                                    Component  8        9      10     11   12                                     ______________________________________                                        Amino fluid                                                                              65       65     65     65   65                                     A1                                                                            TERGITOL   65       40     20     45   27.5                                   TMN-6                                                                         Part I Water                                                                             65       65     65     65   65                                     Acetic Acid                                                                              1        1      1      1    1                                      Part II Water                                                                            130      155    175    150  167.5                                  Haze       100      40     200    80   100                                    pH         5.5      5.5    5.5    5.5  5.5                                    ______________________________________                                    

EXAMPLES 13-17

These examples show the effect of different temperatures of part IIwater and of using different amino fluids(the amounts specified are ingrams):

    ______________________________________                                                   Ex.      Ex.    Ex.     Ex.  Ex.                                   Component  13       14     15      16   17                                    ______________________________________                                        Amino fluid                                                                              65       65     65      0     0                                    A1                                                                            Amino fluid                                                                              0        0      0       65   65                                    A2                                                                            TERGITOL   40       40     40      40   40                                    TMN-6                                                                         Part I Water                                                                             65       65     65      65   65                                    Acetic Acid                                                                              1        1      1       1     1                                    Part II Water                                                                            155      155    115     155   0                                    Part II water                                                                            25       0      75      25   25                                    Temperature                                                                   °C.                                                                    Haze       40       50     50      15   30                                    pH         5.5      5.5    5.5     5.5  nm                                    ______________________________________                                    

EXAMPLES 18-24

These examples show the effect of using fluids with different amineconcentrations at a low amino content (the amounts specified are ingrams):

    ______________________________________                                                 Ex.     Ex.    Ex.   Ex.  Ex.  Ex.   Ex.                             Component                                                                              18      19     20    21   22   23    24                              ______________________________________                                        Amino fluid                                                                             0      50     0     0    0    0     0                               A1                                                                            Amino fluid                                                                             65     15     25    15   0    0     0                               A3                                                                            Amino fluid                                                                             0      0      40    50   65   40    65                              A4                                                                            Amino fluid                                                                             0      0      0     0    0    25    0                               A5                                                                            TERGITOL  40     40     40    40   40   40    40                              TMN-6                                                                         Part I Water                                                                            65     65     65    65   65   65    220                             Acetic Acid                                                                             1      1      1     1    1    1     1                               Part II Water                                                                          155     155    155   155  155  155   0                               Haze     200+    100    80    50   40   60    60                              pH         5.5   5.5    5.5   5.5  5.5  5.5   5.5                             ______________________________________                                         A3 = linear, trimethylsilylterminated, --(CH.sub.2).sub.3 --NH--CH.sub.2      --CH.sub.2 --NH.sub.2 viscosity = 400 centistokes, amine content of 0.07      meq./gr.                                                                      A4 = linear, trimethylsilylterminated, --(CH.sub.2).sub.3 --NH--CH.sub.2      --CH.sub.2 --NH.sub.2 viscosity = 4500-5000 centistokes, amine content of     0.12 meq./gr.                                                                 A5 = linear, trimethylsilylterminated, --(CH.sub.2).sub.3 --NH--CH.sub.2      --CH.sub.2 --NH.sub.2 viscosity = 4500-5000 centistokes, amine content of     0.07 meq./gr.                                                            

EXAMPLE 25

While warming to 70° C., 20 parts of an aminofunctional silicone(linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂pendant, viscosity of 270,000 centistokes, amine content of 0.6 meq/gr.)was mixed with 12.5 parts of TERGITOL TMN-6. Part I water (20 parts) wasthen added dropwise at 70° C. After water addition was complete, 0.5parts of acetic acid was added. The mixture rapidly thickened and becametranslucent. Part II water (47 parts) was then added rapidly with goodagitation. A microemulsion having an ASTM haze number of about 40 wasobtained. Upon heat aging for two weeks at 50° C., the haze increased to50.

EXAMPLE 26

This example shows the effect of adding a buffer to the emulsionformulation.

While warming to 70° C., 20 parts of an aminofunctional silicone(linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂pendant, viscosity of 270,000 centistokes, amine content of 0,6 meq/gr.)was mixed with 12.5 parts of TERGITOL TMN-6. Part I water (20 parts) wasthen added dropwise at 70° C. After water addition was complete, asolution of 2 parts of water, 0.5 parts of acetic acid and 0.25 parts ofsodium acetate was added. The mixture rapidly thickened and becametranslucent. Part II water (44.75) parts) was then added rapidly withgood agitation. A microemulsion having an ASTM haze number of about 10was obtained. Upon heat aging for two weeks at 50° C., the hazeincreased to 40.

EXAMPLE 27

This example shows the effect of varying the amount of Part I water.

While warming to 70° C., 20 parts of an aminofunctional silicone(linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂,viscosity of 270,000 centistokes, amine content of 0.6 meq/gr.) wasmixed with 12.5 parts of TERGITOL TMN-6. Part I water (24 parts,) wasthen added dropwise at 70° C. After water addition was complete,, 0.5parts of acetic acid was added. The mixture rapidly thickened and becametranslucent. This mixture was thinner than that obtained in example 1and was much easier to work with. Part II water (47 parts) was thenadded rapidly with good agitation. A microemulsion having an ASTM hazenumber of under 10 was obtained. Upon heat aging for two weeks at 50°C., the haze increased to 40.

EXAMPLE 28

This example shows the effect of varying the amount of Part I water.

While warming to 70° C., 20 parts of an aminofunctional silicone(linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂pendant, viscosity of 270,000 centistokes, amine content of 0.6 meq/gr.)was mixed with 12.5 parts of TERGITOL TMN-6. Part I water (10 parts) wasthen added dropwise at 70° C. After water addition was complete, 0.5parts of acetic acid was added. The mixture rapidly thickened and becametranslucent. The emulsion was too thick to stir easily with an overheadstirrer. Part II water (57 parts) was then added rapidly with goodagitation. A microemulsion having an ASTM haze number of about 20 wasobtained. Upon heat aging for two weeks at 50° C., the emulsionseparated into two layers.

EXAMPLE 29

This example shows the effect of using a surfactant blend.

While warming to 70° C., 20 parts of an aminofunctional silicone(linear., trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂pendant, viscosity of 270,000 centistokes, amine content of 0.6 meq/gr.)was mixed with 9 parts of TERGITOL TMN-6 and 3 parts of TRITON X-405.Part I water (24 parts) was then added dropwise at 70° C. After wateraddition was complete, 0.5 parts of acetic acid was added. The mixturerapidly thickened and became translucent. Part II water (43.5 parts) wasthen added rapidly with good agitation. A microemulsion having an ASTMhaze number of about 50 was obtained. Upon heat aging for two weeks at50° C., the haze increase to 100.

EXAMPLE 30

This example shows the effect of using a surfactant blend.

While warming to 70° C., 20 parts of an aminofunctional silicone(linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂pendant, viscosity of 270,000 centistokes, amine content of 0.6 meq/gr.)was mixed with 11 parts of TERGITOL TMN-6 and 2.5 parts of TRITON X-405.Part I water (24 parts) was then added dropwise at 70° C. After wateraddition was complete, 0.5 parts of acetic acid was added. The mixturerapidly thickened and became translucent. Part II water (43.5 parts) wasthen added rapidly with good agitation. A microemulsion having an ASTMhaze number of under 10 was obtained. Upon heat aging for two weeks at50° C., the haze did not noticeably increase.

EXAMPLE 31

This example shows the effect of using a surfactant blend

While warming to 70° C., 20 parts of anaminofunctional silicone (linear,trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂, viscosity of270,000 centistokes, amine content of 0.6 meq/gr.) was mixed with 8.5parts of TERGITOL TMN-6 and 1.5 parts of TRITON X-405. Parts 1 water (24parts) was then added dropwise at 70° C. After water addition wascomplete, 0.5 parts of acetic acid was added. The mixture rapidlythickened and became translucent. Part II water (43.5 parts) was thenadded rapidly with good agitation. An emulsion having an ASTM hazenumber of greater than 100 was obtained. The emulsion separated uponheat aging at 50° C.

EXAMPLE 32

This example shows the effect of varying the aminofunctional silicone.

While warming to 70° C., 20 parts of an aminofunctional silicone(linear, trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH2--NH₂,viscosity of 140,000 centistokes, amine content of 0.3 meq/gr.) wasmixed with 12.5 parts of TERGITOL TMN-6. Part I water (20 parts) wasthen added dropwise at 70° C. After water addition was complete, 0.5parts of acetic acid was added. The mixture rapidly thickened and becametranslucent. Part II water (47 parts) was then added rapidly with goodagitation. A microemulsion having an ASTM haze number of about 10 wasobtained. Upon heat aging for two weeks at 50° C., the emulsionseparated into two layers.

EXAMPLE 33

This example shows the effect of using a different fluid. While warmingto 70° C., 20 parts of an aminofunctional silicone (linear,trimethylsilyl terminated, --(CH₂)₃ --NH--CH₂ --CH₂ --NH₂ pendant,viscosity of 140,000 centistokes, amine content of 0.3 meq/gr.) wasmixed with 11 parts of TERGITOL TMN-6 and 2.5 parts of TRITON X-405.Part I water (24 parts) was then added dropwise at 70° C. After wateraddition was complete, 0.5 parts of acetic acid was added. The mixturerapidly thickened and became translucent. Part II water (43.5 parts) wasthen added rapidly with good agitation. A microemulsion having an ASTMhaze number of under 10 was obtained. Upon heat aging for two weeks at50° C., the haze did not noticeably increase.

EXAMPLES 34 THROUGH 38

Examples 34 through 38 were prepared by the technique described inexample 25. A summary of the results obtained on the preparationsexemplified by examples 34 through 38 is presented in the followingTable:

    ______________________________________                                                   EX34  EX35    EX36    EX37  EX38                                   ______________________________________                                        FLUID A      20      20      0     0     0                                    FLUID B      0       0       20    20    0                                    FLUID C      0       0       0     0     20                                   PRIMARY      1.25    8.5     12.5  8.5   12.5                                 SURFACTANT.sup.a                                                              SECONDARY    0       2.5     0     2.5   0                                    SURFACTANT.sup.b                                                              PART I WATER 25      25      25    25                                         BUFFER       3.7     3.7     3.0   3.0   2.5                                  PART II WATER                                                                              38.8    40.3    39.5  41    40                                   INITIAL HAZE 20      20      30    30    40                                   AGING HAZE   40      20      50    40    >100                                 ______________________________________                                         Fluid A = linear, trimethylsilyl terminated, --(CH.sub.2).sub.3               --NH--CH.sub.2 --CH.sub.2 --NH.sub.2, viscosity of 2,000,000 centistokes,     amine content of 0.6 meq/gr.                                                  Fluid B = linear, trimethylsilyl terminated, --(CH.sub.2).sub.3               --NH--CH.sub.2 --CH.sub.2 --NH.sub.2, viscosity of 1,5000,000 csk, amine      content of 0.3 meq/gr.                                                        Fluid C = linear, trimethylsilyl terminated, --(CH.sub.2).sub.3               --NH--CH.sub.2 --CH.sub.2 --NH.sub.2, viscosity of 800,000 csk, amine         content of 0.15 meq/gr.                                                       Primary surfactant = Tergitol TMN6 from Union Carbide                         Secondary surfactant = Triton X405 from Union Carbide                         Bufffer solution is 3 parts water, 0.5 parts acetic acid and 0.2 parts        sodium acetate.                                                               Aging run in a 50 C. oven for 3 weeks in a closed top container under         nitrogen.                                                                

EXAMPLES 39 THROUGH 43 Personal Care Product Formulations

The personal care products exemplified by examples 39 through 43 wereprepared using microemulsions prepared by the process of the presentinvention using a linear trimethylsilyl terminated amino functionalsilicone; the microemulsions had a silicone content of 20 weightpercent. Examples 39 and 40 utilized a microemulsion comprising asilicone fluid having a viscosity of 150 centistokes at 25° C. and anamino content of 0.55 meq./gr. Examples 41 through 43 utilized amicroemulsion comprising a high viscosity amino silicone fluid having aviscosity of 189,000 centistokes at 25° C. and an amino content of 0.30meq./gr.

EXAMPLE

    ______________________________________                                        Material         Amount (wt. %)                                               ______________________________________                                        Deionized water  88.55                                                        Hydroxyethyl Cellulose                                                                         1.0                                                          Cetrimonium Chloride                                                                           3.5                                                          Silicone microemulsion                                                                         6.0                                                          Glydant Plus ®                                                                             0.2                                                          Fragrance        0.75                                                         ______________________________________                                    

The preparative procedure employed was as follows:

With good stirring the hydroxyethyl cellulose was added to the deionizedwater. When complete dispersion was achieved, the Glydant Plus® wasadded and stirred until the mixture was again clear. The aqueous mixturewas heated to 60° C. When the mixture was clear, the cetrimoniumchloride and the silicone microemulsion prepared by the process of thepresent invention were added individually. The mixture was stirred whileallowed to cool. When the temperature was below 40° C., the fragrancewas added. Stirring was continued for approximately 20 minutes after theaddition of the fragrance.

Generally, the optional components may be varied, substituted, oromitted according to the teachings of the art. For example, in order toprevent bacterial growth, preservatives may be added. Additionallyfragrances, pH adjusting agents, antistatic or softening agents,cationic polymers, thickening agents, nonionic polymers such as acrylicacid polymers, neutralizing materials such as triethanolamine,sunscreens, antioxidants, proteins, vitamins, botanical extracts, andthe like may be added.

EXAMPLE 40

A conditioning or 2 in 1 shampoo was prepared from the followingcomponents:

    ______________________________________                                        Material         Amount (wt. %)                                               ______________________________________                                        Deionized water  33.89                                                        Hydroxyethyl Cellulose                                                                         2.0                                                          Ammonium Lauryl Sulfate                                                                        15.38                                                        (as 26% solution)                                                             Ammonium Laureth Sulfate                                                                       21.43                                                        (as 28% solution)                                                             Cocamidopropyl Betaine                                                                         11.43                                                        (as a 35% solution)                                                           Dowicil 200 ®                                                                              0.2                                                          Silicone microemulsion                                                                         5.0                                                          Citric acid      sufficient to adjust to desired pH                           Lauramide DEA    3.5                                                          Cetrimonium Chloride                                                                           6.67                                                         Fragrance        0.5                                                          ______________________________________                                    

The preparative procedure employed was as follows:

The hydroxyethyl cellulose was added to the water and stirred until thehydroxyethyl cellulose was thoroughly solvated. The Dowicil ® was addedand the aqueous mixture was stirred and heated to 60° C. The surfactantswere added in the order listed, individually, followed by stirring untilthe mixture gave a homogeneous appearance. The Lauramide DEA was meltedand added to the mixture. The mixture was then cooled with stirringcontinued during the cooling. When the temperature was below 40° C., thesilicone microemulsion and fragrance were individually added followed bystirring. Mixing was continued for approximately 20 minutes after theaddition of the last component.

EXAMPLE 41

A clear conditioning shampoo formulation was prepared from the followingcomponents:

    ______________________________________                                        Material              Weight Percent                                          ______________________________________                                        Deionized water       31.32                                                   Ammonium Lauryl Sulfate (26% sol'n.)                                                                24.00                                                   Ammonium Laureth Sulfate (28% sol'n.)                                                               14.30                                                   Cocamidopropyl Betaine (35% sol'n.)                                                                 11.43                                                   Amino Silicone Gum Microemulsion                                                                    7.0                                                     Cocamide MEA          2.5                                                     Polysorbate 80        2.5                                                     Lauramide DEA         2.0                                                     Glycerin              2.0                                                     Dimethicone Copolyol  1.0                                                     Guar Hydroxypropyltrimonium Chloride                                                                0.75                                                    Fragrance             0.75                                                    FD&C Yellow #5 (1.0% sol'n.)                                                                        0.25                                                    Methyl Paraben        0.15                                                    Propyl Paraben        0.05                                                    ______________________________________                                    

The methyl and propyl parabens were dissolved in water. The guarhydroxypropyltrimonium chloride was added slowly to the water solutionwith good stirring. When the guar compound was thoroughly solvated, theammonium lauryl sulfate, the ammonium laureth sulfate, and thecocamidopropyl betaine were added individually in order. The solutionwas heated to 65° C. The lauramide DEA and the cocamide MEA were meltedtogether and added to the hot solution with good mixing. The heat wasdiscontinued. The polysorbate 80, glycerin, silicone fluid, and color,and fragrance as desired were mixed together and added to the solutionafter the temperature had cooled to below 45° C. Stirring was continuedfor an additional 10-15 minutes, followed by addition of the siliconegum microemulsion. After addition of the silicone gum microemulsionstirring was continued for an additional 15 minutes.

EXAMPLE 42

A hair conditioner formulation was prepared from the followingcomponents:

    ______________________________________                                        Material             Weight Percent                                           ______________________________________                                        Deionized water      73.40                                                    Silicone Gum Microemulsion                                                                         10.00                                                    Cyclomethicone       5.00                                                     Behentrimonium Methosulfate and                                                                    2.75                                                     Cetearyl Alcohol                                                              Glycerin             2.50                                                     Dimethicone Copolyol 1.75                                                     Stearamidopropyldimethyl amine                                                                     1.50                                                     Cetyl A1cohol        1.50                                                     Pentaerythritol Tetrastearate                                                                      1.30                                                     Methyl Paraben       0.20                                                     Propyl paraben       0.10                                                     Fragrance            as desired                                               ______________________________________                                    

The methyl and propyl parabens were dissolved in water. The solution washeated to 65° C. The behentrimonium methosulfate (and) cetearyl alcohol,stearamidopropyldimethyl amine, and pentaerythritol tetrastearate weremelted together and added to the solution with good stirring. Thesolution was allowed to cool. The glycerin and the dimethicone copolyolwere mixed together along with optional flagrance and added to thesolution after the temperature had dropped below 45° C., with continuedstirring for 15-20 minutes. The silicone gum microemulsion was addedwith stirring for an additional 10-15 minutes. The cyclomethicone wasadded with stirring for an additional 10 minutes.

EXAMPLE 43

A hair conditioning styling mousse was prepared from the followingcomponents:

    ______________________________________                                        Material           Weight Percent                                             ______________________________________                                        Deionized water    79.45                                                      Polyquaternium 11  5.80                                                       Oleth-20           0.75                                                       Silicone Gum Microemulsion                                                                       1.50                                                       Dimethicone Copolyol                                                                             0.50                                                       Propellant hydrocarbons                                                                          12.00                                                      ______________________________________                                    

The water was heated to 45° C., the polyquaternium 11 was added, and thesolution stirred until completely dissolved. The Oleth-20 was then addedwith continued stirring until complete dissolution was obtained. Thesolution was then cooled below 45° C. and the silicone gum microemulsionand dimethicone copolyol were added. Stirring was continued until thesolution was cool. The liquid mousse preparation was then loaded into apressurizable container and pressurized with a mixture of lighthydrocarbons.

Generally, the optional components may be varied, substituted, oromitted according to the teachings of the art. For example, in order toprevent bacterial growth, preservatives may be added. Additionallyfragrances, pH adjusting agents, antistatic or softening agents,cationic polymers, thickening agents, nonionic polymers such as acrylicacid polymers, neutralizing materials such as triethanolamine,sunscreens, antioxidants, proteins, vitamins, botanical extracts, andthe like may be added.

While one of the benefits of using the microemulsions prepared by theprocess of the present invent/on is the ability to prepare clearpersonal care products :having an ASTM haze number below about 100 to150, opacifying or pearlizing agents may be incorporated into thepersonal care product formulations if desired, as demonstrated inexample 42. The microemulsions prepared by the process of the presentinvention provide conditioning benefits to a variety of personal careproducts including, but not limited to, hair coloring compositions,rinses, neutralizing lotions, creams, gels, mousses, aerosols, and pumpsprays.

It is apparent from the foregoing that many other variations andmodifications may be made in the compositions and methods herein beforedescribed without deviating substantially from the process andcompositions of the present invention. Accordingly, the embodiments ofthe present invention herein before described are exemplary only and arenot intended to limit in any fashion or manner the scope of the claimsappended hereto.

What is claimed is:
 1. A translucent oil-in-water microemulsioncomprising:(a) a low amino content microemulsifiable amino siliconehaving an amino content of 0.10 to 3.0 milliequivalents per gram and aviscosity ranging from 100,000 to 10,000,000 centistokes at 25° C., (b)a surfactant having a phase inversion temperature varying from about 45°C. to about 95° C., and (c) water wherein said microemulsion has a meanparticle size ranging from about 0.001 to about 0.050 microns andwhereby said microemulsion has an ASTM D871 haze below about
 150. 2. Themicroemulsion of claim 1 wherein the microemulsifiable silicone is asilicone having the formula:

    M(R.sub.a Q.sub.b SiO.sub.(4-a-b) /2).sub.x (R.sub.c SiO.sub.(4-c) /2).sub.y M

wherein R is a hydrocarbon radical having from 1 to about 6 carbonatoms, Q is a polar radical having the general formula --R¹ HZ, whereinR¹ is a divalent linking group bound to hydrogen and a radical Z whereinR¹ is comprised of carbon and hydrogen atoms; carbon, hydrogen andoxygen atoms, or carbon, hydrogen and nitrogen atoms; and Z is an aminocontaining radical having the formula:

    --N(CH.sub.2).sub.z (CH.sub.2).sub.zz NH

wherein z is one or greater and zz is zero or greater subject to thelimitation such that when zz is zero Z has the formula:

    --NH(CH.sub.2).sub.z NH.sub.2

wherein z is one or greater; a ranges from about 0 to about 2, b rangesfrom about 1 to about 3 such that a +b is less than or equal to 3, and cis a number in the range of from about 1 to about 3; and x is a numberin the range of from 5 to about 2,000, and y is a number in the range offrom about 800 to about 10,000, and M is a silicone endstopping group.3. The microemulsion of claim 2 herein the microemulsifiable siliconefurther comprises a silicone having the formula:

    (CH.sub.3).sub.3 SiO[(CH.sub.3)(C.sub.3 H.sub.6 NH.sub.2 C.sub.2 H.sub.4 NH.sub.2)SiO].sub.x [(CH.sub.3).sub.2 SiO].sub.y Si(CH.sub.3).sub.3

wherein x is a number in the range of from about 5 to about 2,000 and yis a number in the range from about 800 to about 10,000.
 4. Atranslucent oil-in-water microemulsion consisting essentially of:(a) alow amino content microemulsifiable silicone having an amino content of0.10 to 3.0 milliequivalents per gram and a viscosity ranging from100,000 to 10,000,000 centistokes at 25° C., (b) a surfactant having aphase inversion temperature varying from about 45° to about 95° C., and(c) water wherein said microemulsion has a mean particle size rangingfrom about 0.001 to about 0.050 microns and whereby said microemulsionhas an ASTM D871 haze below about
 150. 5. A process for preparing amicroemulsion comprising:(a) preparing a blend of silicones comprising alow amino content microemulsifiable silicone having an amino content of0.10 to 3.0 milliequivalents per gram and a viscosity ranging from100,000 to 10,000,000 centistokes at 25° C. said microemulsifiablesilicone having the formula:

    M(R.sub.a Q.sub.b SiO.sub.(4-a-b) /2).sub.x (R.sub.c SiO.sub.(4-c) /2).sub.y M

wherein R is a hydrocarbon or hydrocarbon radical having from 1 to about6 carbon atoms, Q is a polar radical having the general formula --R¹ HZ,wherein R¹ is a divalent linking group bound to hydrogen and a radical Zwherein R¹ is comprised of carbon and hydrogen atoms; carbon, hydrogenand oxygen atoms, or carbon, hydrogen and nitrogen atoms; and Z is anamino containing radical having the formula:

    --N(CH.sub.2).sub.z (CH.sub.2).sub.zz NH

wherein z is one or greater and zz is zero or greater subject to thelimitation such that when zz is zero Z has the formula:

    --NH(CH.sub.2).sub.z NH.sub.2

wherein z is one or greater; a ranges from about 0 to about 2, b rangesfrom about 1 to about 3 such that a+b is less than or equal to 3, and cis a number in the range of from about 1 to about 3; and x is a numberin the range of from 5 to about 2,000, and y is a number in the range offrom about 800 to about 10,000, and M is a silicone endstopping group;(b) adding a surfactant having a phase inversion temperature rangingfrom about 450° C. to about 95° C.; (c) heating said silicone and saidsurfactant to a temperature ranging from about 45° C. to 95° C.; (d)adding part I water; (e) adding an acid; and (f) adding part II waterwherein said microemulsion has a mean particle size ranging from about0.001 to about 0.050 microns and whereby said microemulsion has an ASTMD871 haze below about
 150. 6. The method of claim 5 wherein steps (d)and (e) are performed substantially simultaneously.
 7. The method ofclaim 5 wherein the acid of step (e) is dissolved in the water of step(d) to produce an acid solution and said acid solution is added to themixture of (a) and (b).
 8. The method of claim 5 wherein the amount ofsilicone ranges from 10 to 30 parts per hundred of the total compositionof the microemulsion.
 9. The method of claim 5 herein the amount ofsurfactant ranges from about 1 to 20 parts per hundred of the totalcomposition of the microemulsion.
 10. The method of claim 5 wherein theamount of part I water by weight is substantially equal to the weight ofsaid silicone.
 11. The method of claim 5 wherein the amount or part IIwater by weight ranges from about 40 to about 90 parts per hundred ofthe total composition of the microemulsion.
 12. The method of claim 5wherein the acid is selected from the group consisting of acetic,hydrochloric, hypophosphorous, lactic, propionic, glycolic, formic, andnitric acids.
 13. The method of claim 5 wherein the microemulsifiablesilicone has the formula:

    (CH.sub.3).sub.3 SiO[(CH.sub.3)(C.sub.3 H.sub.6 NH.sub.2 C.sub.2 H.sub.4 NH.sub.2)SiO].sub.x [(CH.sub.3).sub.2 SiO].sub.y Si(CH.sub.3).sub.3

wherein x is a number in the range of from about 5 to about 2,000, and yis a number in the range from about 800 to about 10,000.
 14. A personalcare product comprising the microemulsion of claim 1 whereby saidmicroemulsion has an ASTM D871 haze below about
 100. 15. The personalcare product of claim 14 wherein the personal care product is aconditioner wherein the microemulsion is present in an amount rangingfrom about 5 weight percent to about 15 weight percent.
 16. The personalcare product of claim 14 wherein the personal care product is a 2 in 1shampoo wherein the microemulsion is present in an amount ranging fromabout 2 weight percent to about 7 weight percent.
 17. The personal careproduct of claim 14 wherein the personal care product is a fixativewherein the microemulsion is present in an amount ranging from about 2weight percent to about 10 weight percent.